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Pesquisa : E05.196 [Categoria DeCS]
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[PMID]:29431332
[Au] Autor:Iakubova IS; Dadaly YV; Mel'tser AV; Alikbayeva LA; Zhirnov AY; Andreyeva MA; Gorshkova MP; Antonova MS
[Ti] Título:[Methodical issues of the monitoring for ammonium in indoors air].
[So] Source:Gig Sanit;95(10):917-22, 2016.
[Is] ISSN:0016-9900
[Cp] País de publicação:Russia (Federation)
[La] Idioma:rus
[Ab] Resumo:Introduction. To perform mass studies of the indoors air environment of the ammonium content the actual issues are the shortening of the sampling time and material costs for their implementation, reduction of adverse effects of ammonium with keeping of the objectivity of results. Aim. The elaboration of the method of short-term air sampling for indoors ammonium and comparative assessment ofdifferent methods of sampling in the course of modeling and field tests. Materials and Methods. Air sampling for ammonium was carried out according to the developed program and standard method, under the average daily 4-fold taking according to State Standards (GOST) 17.2.3.01-86 andRD 52.04.186-89. The evaluation of the significance of deviations of analysis results was carried out in accordance with GOST R ISO 5725-6-2002 and Recommendations of the Interstate Standardization RMG - 61-2003. Results. There were executed model and field tests of air sampling for ammonium according to the standard method and the program of short-term sampling. There were obtained significantly comparable results of ammonium content in the indoor air in the course of model and field tests. Conclusions. Sampling according to the developed program has a number of advantages, including: the shortening of sampling time, material costs, increasing in productivity in the analysis of indoor airfor the ammonium content. The execution oftest sampling according to the developed program allows to reduce the time of ammonium exposure to personnel carrying out the test sampling.
[Mh] Termos MeSH primário: Poluentes Atmosféricos/análise
Poluição do Ar em Ambientes Fechados/análise
Compostos de Amônio/análise
[Mh] Termos MeSH secundário: Poluição do Ar em Ambientes Fechados/prevenção & controle
Técnicas de Química Analítica/métodos
Técnicas de Química Analítica/normas
Monitoramento Ambiental/métodos
Seres Humanos
Exposição por Inalação/análise
Exposição por Inalação/prevenção & controle
Reprodutibilidade dos Testes
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Air Pollutants); 0 (Ammonium Compounds)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:180213
[St] Status:MEDLINE


  2 / 9456 MEDLINE  
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[PMID]:29343296
[Au] Autor:Seljetun KO; Eliassen E; Karinen R; Moe L; Vindenes V
[Ad] Endereço:Department of Companion Animal Clinical Sciences, Faculty of Veterinary Medicine, Norwegian University of Life Sciences (NMBU), P.O. Box 8146 Dep, 0033, Oslo, Norway. kristin.opdal.seljetun@nmbu.no.
[Ti] Título:Quantitative method for analysis of six anticoagulant rodenticides in faeces, applied in a case with repeated samples from a dog.
[So] Source:Acta Vet Scand;60(1):3, 2018 Jan 17.
[Is] ISSN:1751-0147
[Cp] País de publicação:England
[La] Idioma:eng
[Ab] Resumo:BACKGROUND: Accidental poisoning with anticoagulant rodenticides is not uncommon in dogs, but few reports of the elimination kinetics and half-lives in this species have been published. Our objectives were to develop and validate a new method for the quantification of anticoagulant rodenticides in canine blood and faeces using reversed phase ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and apply the method on a case of anticoagulant rodenticide intoxication. RESULTS: Sample preparation was liquid-liquid extraction. Six anticoagulant rodenticides were separated using a UPLC BEH C -column with a mobile phase consisting of 5 mM ammonium formate buffer pH 10.2 and methanol. MS/MS detection was performed with positive electrospray ionization and two multiple reaction monitoring transitions. The limits of quantification were set at the levels of the lowest calibrator (1.5-2.7 ng/mL or ng/g). The method was successfully applied to a case from a dog accidentally poisoned with anticoagulant rodenticide. Coumatetralyl and brodifacoum concentrations were determined from serial blood and faecal samples. A terminal half-life of at least 81 days for coumatetralyl in blood was estimated, which is longer than previous reported in other species. A slow elimination of brodifacoum from the faeces was found, with traces still detectable in the faeces at day 513. CONCLUSIONS: This study offers a new method of detection and quantification of six frequently used anticoagulant rodenticides in canine faeces. Such drugs might cause serious health effects and it is important to be able to detect these drugs, to initiate proper treatment. The very long elimination half-lives detected in our study is important to be aware of in assessment of anticoagulant rodenticide burden to the environment.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Fezes/química
Rodenticidas/análise
Rodenticidas/envenenamento
[Mh] Termos MeSH secundário: Animais
Anticoagulantes/análise
Anticoagulantes/sangue
Anticoagulantes/envenenamento
Técnicas de Química Analítica/normas
Cromatografia Líquida de Alta Pressão
Cães
Meia-Vida
Limite de Detecção
Rodenticidas/sangue
Espectrometria de Massas em Tandem
[Pt] Tipo de publicação:JOURNAL ARTICLE; VALIDATION STUDIES
[Nm] Nome de substância:
0 (Anticoagulants); 0 (Rodenticides)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:180119
[St] Status:MEDLINE
[do] DOI:10.1186/s13028-018-0357-9


  3 / 9456 MEDLINE  
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[PMID]:29276081
[Au] Autor:Uchiyama S; Sasaki T; Ishihara R; Fujiwara K; Sugo T; Umeno D; Saito K
[Ad] Endereço:Department of Applied Chemistry and Biotechnology, Chiba University, 1-33 Yayoi, Inage, Chiba 263-8522, Japan.
[Ti] Título:High-resolution separation of neodymium and dysprosium ions utilizing extractant-impregnated graft-type particles.
[So] Source:J Chromatogr A;1533:10-16, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:An efficient method for rare metal recovery from environmental water and urban mines is in high demand. Toward rapid and high-resolution rare metal ion separation, a novel bis(2-ethylhexyl) phosphate (HDEHP)-impregnated graft-type particle as a filler for a chromatography column is proposed. To achieve rapid and high-resolution separation, a convection-flow-aided elution mode is required. The combination of 35 µm non-porous particles and a polymer-brush-rich particle structure minimizes the distance from metal ion binding sites to the convection flow in the column, resulting in minimized diffusional mass transfer resistance and the convection-flow-aided elution mode. The HDEHP-impregnated graft-type non-porous-particle-packed cartridge developed in this study exhibited a higher separation performance for model rare metals, neodymium (III) and dysprosium (III) ions, and a narrower peak at a higher linear velocity, than those of previous HDEHP-impregnated fiber-packed and commercially available Lewatit VP OC 1026-packed cartridges.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Disprósio/isolamento & purificação
Neodímio/isolamento & purificação
[Mh] Termos MeSH secundário: Cromatografia
Difusão
Disprósio/química
Íons/química
Íons/isolamento & purificação
Metais/química
Neodímio/química
Polímeros/química
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Ions); 0 (Metals); 0 (Polymers); 1D4N45714Q (Dysprosium); 2I87U3734A (Neodymium)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171226
[St] Status:MEDLINE


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[PMID]:29249536
[Au] Autor:Serroukh S; Huber P; Lallam A
[Ad] Endereço:Centre Technique du Papier, Domaine universitaire - CS, 90251 - 38044 Grenoble, France; Université de Haute Alsace, 18 Rue des Frères Lumière, 68093 Mulhouse, France. Electronic address: serroukhsonia@hotmail.com.
[Ti] Título:Adsorption behavior of optical brightening agent on microfibrillated cellulose studied through inverse liquid chromatography: The need to correct for axial dispersion effect.
[So] Source:J Chromatogr A;1533:17-29, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:Inverse liquid chromatography is a technique for studying solid/liquid interaction and most specifically for the determination of solute adsorption isotherm. For the first time, the adsorption behaviour of microfibrillated cellulose was assessed using inverse liquid chromatography. We showed that microfibrillated cellulose could adsorb 17 mg/g of tetrasulfonated optical brightening agent in typical papermaking conditions. The adsorbed amount of hexasulfonated optical brightening agent was lower (7 mg/g). The packing of the column with microfibrillated cellulose caused important axial dispersion (D = 5e-7 m²/s). Simulation of transport phenomena in the column showed that neglecting axial dispersion in the analysis of the chromatogram caused significant error (8%) in the determination of maximum adsorbed amount. We showed that conventional chromatogram analysis technique such as elution by characteristic point could not be used to fit our data. Using a bi-Langmuir isotherm model improved the fitting, but did not take into account axial dispersion, thus provided adsorption parameters which may have no physical significance. Using an inverse method with a single Langmuir isotherm, and fitting the transport equation to the chromatogram was shown to provide a satisfactory fitting to the chromatogram data. In general, the inverse method could be recommended to analyse inverse liquid chromatography data for column packing with significant axial dispersion (D > 1e-7 m²/s).
[Mh] Termos MeSH primário: Celulose/química
Técnicas de Química Analítica/instrumentação
Técnicas de Química Analítica/métodos
Cromatografia Líquida
Eliminação de Resíduos Líquidos/métodos
[Mh] Termos MeSH secundário: Adsorção
Resíduos Industriais
Modelos Químicos
Papel
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Industrial Waste); 9004-34-6 (Cellulose)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171219
[St] Status:MEDLINE


  5 / 9456 MEDLINE  
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[PMID]:29248346
[Au] Autor:Wang Y; Tong Y; Xu X; Zhang L
[Ad] Endereço:College of Chemistry, Liaoning University, Shenyang 110036, China.
[Ti] Título:Metal-organic framework-derived three-dimensional porous graphitic octahedron carbon cages-encapsulated copper nanoparticles hybrids as highly efficient enrichment material for simultaneous determination of four fluoroquinolones.
[So] Source:J Chromatogr A;1533:1-9, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:A unique 3D porous Cu@graphitic octahedron carbon cages were constructed by rapid room-temperature synthesis of a Cu-based metal-organic framework (MOF) with further pyrolysis in N , which exhibited good enrichment ability for four fluoroquinolones (FQs) due to their superior chemical affinities to the target analytes. Applied Cu@graphitic octahedron carbon cages as adsorbent, a dispersive solid phase extraction (DSPE) method combined with HPLC was developed for detecting four FQs in real samples. Various parameters affecting residues FQs extraction efficiency were inquired in more detail. Under optimal conditions, the extraction recoveries of four FQs in chicken muscle, fish tissue, seawater and river water samples were in the range of 81.3∼104.3% and the RSDs (n = 5) were less than 5.2%. This method was successfully used to the determination of FQs in real samples.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Cobre/química
Fluoroquinolonas/análise
Grafite/química
Estruturas Metalorgânicas/química
Nanopartículas/química
[Mh] Termos MeSH secundário: Anti-Infecciosos
Cromatografia Líquida de Alta Pressão
Porosidade
Extração em Fase Sólida
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Anti-Infective Agents); 0 (Fluoroquinolones); 0 (Metal-Organic Frameworks); 7782-42-5 (Graphite); 789U1901C5 (Copper)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171218
[St] Status:MEDLINE


  6 / 9456 MEDLINE  
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[PMID]:29248344
[Au] Autor:Tong C; Peng M; Tong R; Ma R; Guo K; Shi S
[Ad] Endereço:College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, PR China.
[Ti] Título:Use of an online extraction liquid chromatography quadrupole time-of-flight tandem mass spectrometry method for the characterization of polyphenols in Citrus paradisi cv. Changshanhuyu peel.
[So] Source:J Chromatogr A;1533:87-93, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC-DAD-QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction of Citrus paradisi cv. Changshanhuyu (Changshanhuyu) peel, OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of twenty-two secondary metabolites were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and nine of them were discovered in Changshanhuyu peel for the first time to our knowledge. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Cromatografia Líquida de Alta Pressão
Citrus paradisi/química
Polifenóis/química
Espectrometria de Massas em Tandem
[Mh] Termos MeSH secundário: Produtos Biológicos/química
Frutas/química
Polifenóis/isolamento & purificação
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Biological Products); 0 (Polyphenols)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171218
[St] Status:MEDLINE


  7 / 9456 MEDLINE  
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[PMID]:29241957
[Au] Autor:Luo YD; Zhang QL; Yao SJ; Lin DQ
[Ad] Endereço:Key Laboratory of Biomass Chemical Engineering of Ministry of Education, College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, China.
[Ti] Título:Evaluation of adsorption selectivity of immunoglobulins M, A and G and purification of immunoglobulin M with mixed-mode resins.
[So] Source:J Chromatogr A;1533:77-86, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:This study investigated adsorption selectivity of immunoglobulin M (IgM), immunoglobulin A (IgA) and immunoglobulin (IgG) on four mixed-mode resins with the functional ligands of 4-mercatoethyl-pyridine (MEP), 2-mercapto-1-methylimidazole (MMI), 5-aminobenzimidazole (ABI) and tryptophan-5-aminobenzimidazole (W-ABI), respectively. IgM purification processes with mixed-mode resins were also proposed. All resins showed typical pH-dependent adsorption, and high adsorption capacity was found at pH 5.0-8.0 with low adsorption capacity under acidic conditions. Meanwhile, high selectivity of IgM/IgA and IgM/IgG was obtained with ABI-4FF and MMI-4FF resins at pH 4.0-5.0, which was used to develop a method for IgM, IgA and IgG separation by controlling loading and elution pH. Capture of monoclonal IgM from cell culture supernatant with ABI-4FF resins was studied and high purity (∼99%) and good recovery (80.8%) were obtained. Moreover, IgM direct separation from human serum with combined two-step chromatography (ABI-4FF and MMI-4FF) was investigated, and IgM purity of 65.2% and a purification factor of 28.3 were obtained after optimization. The antibody activity of IgM was maintained after purification. The results demonstrated that mixed-mode chromatography with specially-designed ligands is a promising way to improve adsorption selectivity and process efficiency of IgM purification from complex feedstock.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Cromatografia
Imunoglobulina M/isolamento & purificação
Resinas Sintéticas/química
[Mh] Termos MeSH secundário: Adsorção
Células Cultivadas
Técnicas de Química Analítica/normas
Seres Humanos
Interações Hidrofóbicas e Hidrofílicas
Imunoglobulina A/metabolismo
Imunoglobulina G/metabolismo
Imunoglobulina M/metabolismo
Ligantes
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Immunoglobulin A); 0 (Immunoglobulin G); 0 (Immunoglobulin M); 0 (Ligands); 0 (Resins, Synthetic)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171216
[St] Status:MEDLINE


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[PMID]:29229336
[Au] Autor:Panda SK; Muller H; Al-Qunaysi TA; Koseoglu OR
[Ad] Endereço:Saudi Aramco, Research & Development Center, 31311, Dhahran, Saudi Arabia. Electronic address: saroj.panda@aramco.com.
[Ti] Título:Determination of heavy polycyclic aromatic hydrocarbons by non-aqueous reversed phase liquid chromatography: Application and limitation in refining streams.
[So] Source:J Chromatogr A;1533:30-37, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:The heavy polycyclic aromatic hydrocarbons (HPAHs) cause detrimental effects to hydrocracker operations by deactivating the catalysts and depositing in the downstream of the reactor/ exchangers. Therefore, it is essential to continuously monitor the accumulation of HPAHs in a hydrocracker unit. To accurately measure the concentration of HPAHs, the development of a fast and reliable analytical method is inevitable. In this work, an analytical method based on non-aqueous reversed phase chromatography in combination with high resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was developed. As a first step, five different types of stationary phases were evaluated for the separation of HPAHs in non-aqueous mode and the best suited phase was further used for the fractionation of HPAHs in a fractionator bottom sample obtained from a refinery hydrocracker unit. The eight major fractions or peaks obtained from the separation were further characterized by UV spectroscopy and FT-ICR MS and the compounds in the fractions were tentatively confirmed as benzoperylene, coronene, methylcoronene, naphthenocoronene, benzocoronene, dibenzoperylene, naphthocoronene and ovalene. The developed liquid chromatography method can be easily adapted in a refinery laboratory for the quantitation of HPAHs in hydrocracking products. The method was further tested to check the interference of sulfur aromatics and/or large alkylated aromatic hydrocarbons on the determination of HPAHs in hydrocracking products.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Cromatografia de Fase Reversa
Espectrometria de Massas
Indústria de Petróleo e Gás/métodos
Hidrocarbonetos Aromáticos Policíclicos/análise
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Polycyclic Aromatic Hydrocarbons)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171213
[St] Status:MEDLINE


  9 / 9456 MEDLINE  
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[PMID]:29229331
[Au] Autor:Großhans S; Wang G; Fischer C; Hubbuch J
[Ad] Endereço:Karlsruhe Institute of Technology (KIT), Institute of Process Engineering in Life Sciences, Section IV: Biomolecular Separation Engineering, Karlsruhe, Germany.
[Ti] Título:An integrated precipitation and ion-exchange chromatography process for antibody manufacturing: Process development strategy and continuous chromatography exploration.
[So] Source:J Chromatogr A;1533:66-76, 2018 Jan 19.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:In the past decades, research was carried out to find cost-efficient alternatives to Protein A chromatography as a capture step in monoclonal antibody (mAb) purification processes. In this work, polyethylene glycol (PEG) precipitation has shown promising results in the case of mAb yield and purity. Especially with respect to continuous processing, PEG precipitation has many advantages, like low cost of goods, simple setup, easy scalability, and the option to handle perfusion reactors. Nevertheless, replacing Protein A has the disadvantage of renouncing a platform unit operation as well. Furthermore, PEG precipitation is not capable of reducing high molecular weight impurities (HMW) like aggregates or DNA. To overcome these challenges, an integrated process strategy combining PEG precipitation with cation-exchange chromatography (CEX) for purification of a mAb is presented. This work discusses the process strategy as well as the associated fast, easy, and material-saving process development platform. These were implemented through the combination of high-throughput methods with empirical and mechanistic modeling. The strategy allows the development of a common batch process. Additionally, it is feasible to develop a continuous process. In the presented case study, a mAb provided from cell culture fluid (HCCF) was purified. The precipitation and resolubilization conditions as well as the chromatography method were optimized, and the mutual influence of all steps was investigated. A mAb yield of over 95.0% and a host cell protein (HCP) reduction of over 99.0% could be shown. At the same time, the aggregate level was reduced from 3.12% to 1.20% and the DNA level was reduced by five orders of magnitude. Furthermore, the mAb was concentrated three times to a final concentration of 11.9mg/mL.
[Mh] Termos MeSH primário: Anticorpos Monoclonais/isolamento & purificação
Técnicas de Química Analítica/métodos
Cromatografia por Troca Iônica
[Mh] Termos MeSH secundário: Anticorpos Monoclonais/biossíntese
Técnicas de Química Analítica/economia
Polietilenoglicóis/química
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Antibodies, Monoclonal); 30IQX730WE (Polyethylene Glycols)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180227
[Lr] Data última revisão:
180227
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171213
[St] Status:MEDLINE


  10 / 9456 MEDLINE  
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[PMID]:29229335
[Au] Autor:Liu YE; Huang LQ; Luo XJ; Tan XX; Huang CC; Corella PZ; Mai BX
[Ad] Endereço:State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Resources Utilization and Protection, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, 510640, PR China; University of Chinese Academy of Sciences, Beijing, 100049, PR China.
[Ti] Título:Determination of organophosphorus flame retardants in fish by freezing-lipid precipitation, solid-phase extraction and gas chromatography-mass spectrometry.
[So] Source:J Chromatogr A;1532:68-73, 2018 Jan 12.
[Is] ISSN:1873-3778
[Cp] País de publicação:Netherlands
[La] Idioma:eng
[Ab] Resumo:An analytical method has been developed for measuring 12 organophosphorus flame retardants (PFRs) in fish tissue samples. After the Soxhlet extraction of PFRs with dichloromethane. The experimental parameters of the clean-up were systematically optimized. Methanol was found to be a more effective solvent than acetonitrile used in freezing-lipid precipitation. Methanol (5%) in ultrapure water, was finally selected to perform solid-phase extraction (SPE, Oasis HLB cartridge), with mean lipid removal efficiency of 94% after freezing-lipid precipitation. Further purification followed by 200mg of Z-Sep and C18 dispersant to eliminate the remaining interferences. Quantification was performed using gas chromatography-mass spectrometry in selective ion monitoring mode. The recovery, precision, and the method detection limits (MDLs) were verified by spiking experiments. All chemicals except triethyl phosphate (TEP) showed satisfactory recoveries in the range of 73-107% and 56-108% in the spiked blanks samples and spiked fish tissue samples, respectively. MDLs for PFRs in the biological samples ranged from 0.004 to 0.059ng/g. The proposed method successfully applied to the determination of PFRs in real fish samples with recoveries of four internal standards varying from 75 to 97%. The results demonstrated that the proposed method is highly effective for analyzing PFRs in fish samples.
[Mh] Termos MeSH primário: Técnicas de Química Analítica/métodos
Peixes
Retardadores de Chama/análise
Congelamento
Cromatografia Gasosa-Espectrometria de Massas
Extração em Fase Sólida
[Mh] Termos MeSH secundário: Animais
Técnicas de Química Analítica/instrumentação
Limite de Detecção
Lipídeos/química
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Flame Retardants); 0 (Lipids)
[Em] Mês de entrada:1802
[Cu] Atualização por classe:180222
[Lr] Data última revisão:
180222
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171213
[St] Status:MEDLINE



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